CN102950537B - It is used for the method for chemically machinery polished copper - Google Patents
It is used for the method for chemically machinery polished copper Download PDFInfo
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- CN102950537B CN102950537B CN201210289359.6A CN201210289359A CN102950537B CN 102950537 B CN102950537 B CN 102950537B CN 201210289359 A CN201210289359 A CN 201210289359A CN 102950537 B CN102950537 B CN 102950537B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
- H01L21/7684—Smoothing; Planarisation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/31051—Planarisation of the insulating layers
- H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
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- Manufacturing & Machinery (AREA)
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- Power Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
Disclose a kind of method being used for chemically machinery polished copper. It is specifically related to a kind of use the chemical-mechanical polishing compositions of degree of imperfection non-selective, low that the substrate comprising copper is carried out the method for chemically machinery polished.
Description
Technical field
The present invention relates to the method for substrate being carried out chemically machinery polished. In particular, it relates to be used for being carried out by the semiconductor chip comprising copper-connection the method for chemically machinery polished.
Technical background
Copper, because of the anti-electronic migration ability of its relatively low resistivity and raising, is the selection of the interconnection material for semiconductor wafer Integrated Solution at present. Consider and adopt plasma body to carry out copper etching relevant difficulty, usually carry out manufactured copper interconnection by embedded technology (damascene). In the embedded structure of routine, etched recesses or perforation in the dielectric layer; Again blocking material (usual Ta, TaN) and seed copper material are deposited in this groove or perforation; Again by electroplating deposition copper body. The copper of deposition fills the region (e.g., groove or perforation) needed, and spreads out the wafer area of surrounding. Remove the copper product of (overload) not again with chemically machinery polished (CMP), and make wafer surface planing.
Conventional copper CMP normally multistep technique. The usual the first step uses copper has the high polishing composition removing rate selectivities (relative to blocking material), removes, from wafer surface, (overload) copper that big block do not want to promote fast. The polishing composition of described highly selective is designed to stop over the barrier layer polishing. But, described high-copper optionally the first step polishing step to cause being positioned at the layers of copper of groove or perforation polished, cause the effect being called depression. Usual 2nd step uses another kind of polishing composition (stop preparation) to be used for removing blocking material from wafer surface. In common low selectivity slurries (LSS) Integrated Solution, selected stop preparation is designed to that copper is shown non-selective (relative to blocking material) and to improve processing leeway and reduces depression. Such as, periodically, the 3rd step (polishing step) is implemented to improve the degree of imperfection of glazed surface.
Carrying out in chemically machinery polished to copper, in view of the relative softness of copper, improving defect performance is a kind of difficult challenge. Defect mainly various cut and the jarring marks that copper CMP is relevant. Owing to relating to relevant loss of yield and reliability, the defective improved in copper CMP has special interest.
No. 2008/0148652nd, the United States Patent (USP) of Siddiqui etc. discloses a kind of scheme for improvement of the degree of imperfection in copper CMP that it is said. Siddiqui etc. disclose a kind of composition and are used for the methods involving carrying out chemically machinery polished containing copper base, it is claimed and copper obtains low defect level in copper CMP process, wherein, described composition comprises the colloidal silica of not containing water-soluble polymkeric substance silicate substantially.
But, the method for copper defect performance that this area continues to need to develop new chemical mechanical polishing composition and can be improved.
Summary of the invention
The present invention provides a kind of method being used for being carried out by substrate chemically machinery polished, and the method comprises: providing substrate, wherein, described substrate comprises copper; Thering is provided a kind of chemical mechanical polishing pulp composition, it comprises following component as initial component: water; The abrasive material of 0.1-20 weight %; The complexing agent of 0.01-15 weight %; The inhibitor of 0.02-5 weight %; The P contained compound of 0.01-5 weight %; The Polyvinylpyrolidone (PVP) of 0.001-3 weight %; > Histidine of 0.1-1 weight %; > the guanidine class thing of 0.1-1 weight %, wherein, described guanidine class thing is selected from guanidine, guanidine derivative, guanidine salt and their mixture; The optional oxygenant of 0-25 weight %; The optional flow agent of 0-0.1 weight %; The optional biocide of 0-0.01 weight %; Optional pH adjusting agent, wherein, the pH value of described chemical mechanical polishing pulp composition is 9-11; The chemical mechanical polishing pads with glazed surface is provided; Interface between described chemical mechanical polishing pads and substrate or near interface, be assigned on described chemical mechanical polishing pads by described chemical mechanical polishing pulp composition; And set up dynamically contact with the interface of the down force of 0.69-34.5 kPa between the glazed surface and substrate of chemical mechanical polishing pads; Described substrate is polished; And from substrate remove a part copper.
Present invention also offers a kind of method being used for being carried out by substrate chemically machinery polished, the method comprises: providing substrate, described substrate comprises copper; Thering is provided a kind of chemical mechanical polishing pulp composition, it comprises following component as initial component: water; The abrasive material of 0.5-15 weight %, described abrasive material is mean particle size is the colloidal silica abrasive of 25-75 nanometer; The complexing agent of 0.1-1 weight %, described complexing agent is citric acid; The inhibitor of 0.05-2 weight %, described inhibitor is benzotriazole; The P contained compound of 0.05-3 weight %, described P contained compound is phosphoric acid; The Polyvinylpyrolidone (PVP) of 0.05-1.5 weight %, the weight-average molecular weight of described Polyvinylpyrolidone (PVP) is 2500-50000; The Histidine of 0.25-1 weight %; The guanidine class thing of 0.25-1 weight %, described guanidine class thing is selected from guanidine, guanidine derivative, guanidine salt and their mixture; The oxygenant of 0.1-10 weight %, described oxygenant is H2O2; The flow agent of 0.01-0.1 weight %, described flow agent is ammonium chloride; The biocide of 0.001-0.01 weight %; With the pH adjusting agent of 0.1-1 weight %, described pH adjusting agent is potassium hydroxide; The chemical mechanical polishing pads with glazed surface is provided; Interface between described chemical mechanical polishing pads and substrate or near interface, be assigned on described chemical mechanical polishing pads by described chemical mechanical polishing pulp composition; And set up dynamically contact with the interface of the down force of 0.69-34.5 kPa between the glazed surface and substrate of chemical mechanical polishing pads; Described substrate is polished; And from substrate remove a part copper; Further, on the polishing machine of 200 millimeters under following operational condition, the copper of described chemical-mechanical polishing compositions removes speed/ minute, and size after polishing > SP1 defect counting��200 of 0.1 micron: platen rotating speed 93 revs/min, carrier velocity 87 revs/min, flow 300 ml/min of chemical-mechanical polishing compositions, apply the nominal down force of 11.7 kPas, described polishing machine uses chemical mechanical polishing pads, and it comprises the non-woven subpad of the polyurethane polishing layer containing the hollow core particulate of polymkeric substance and polyurethane impregnated.
Present invention also offers a kind of method being used for being carried out by substrate chemically machinery polished, the method comprises: providing substrate, described substrate comprises copper; Thering is provided a kind of chemical mechanical polishing pulp composition, it comprises following component as initial component: water; The abrasive material of 10-15 weight %, described abrasive material is mean particle size is the colloidal silica abrasive of 25-75 nanometer; The complexing agent of 0.01-0.5 weight %, described complexing agent is citric acid; The inhibitor of 0.05-1 weight %, described inhibitor is benzotriazole; The P contained compound of 0.05-0.2 weight %, described P contained compound is phosphoric acid; The Polyvinylpyrolidone (PVP) of 0.1-1 weight %, the weight-average molecular weight of described Polyvinylpyrolidone (PVP) is 12000-20000; The Histidine of 0.25-0.6 weight %; The Guanidinium hydrochloride of 0.25-0.6 weight %; The oxygenant of 0.1-5 weight %, described oxygenant is H2O2; The flow agent of 0.01-0.05 weight %, described flow agent is ammonium chloride; The biocide of 0.001-0.01 weight %; With the pH adjusting agent of 0.1-1 weight %, described pH adjusting agent is potassium hydroxide; It is included in chemical-mechanical polishing compositions as the Histidine of initial component and the quality of Guanidinium hydrochloride and has��the difference of 10%; The chemical mechanical polishing pads with glazed surface is provided; Interface between described chemical mechanical polishing pads and substrate or near interface, be assigned on described chemical mechanical polishing pads by described chemical mechanical polishing pulp composition; And set up dynamically contact with the interface of the down force of 0.69-34.5 kPa between the glazed surface and substrate of chemical mechanical polishing pads; Described substrate is polished; And from substrate remove a part copper; Further, on the polishing machine of 200 millimeters under following operational condition, the copper of described chemical-mechanical polishing compositions removes speed/ minute, and size after polishing > SP1 defect counting��200 of 0.1 micron: platen rotating speed 93 revs/min, carrier velocity 87 revs/min, flow 300 ml/min of chemical-mechanical polishing compositions, apply the nominal down force of 11.7 kPas, described polishing machine uses chemical mechanical polishing pads, and it comprises the non-woven subpad of the polyurethane polishing layer containing the hollow core particulate of polymkeric substance and polyurethane impregnated.
Embodiment
Cmp method of the present invention is applicable to the polishing containing copper base, particularly comprises the polishing of the semiconductor wafer of copper-connection. The copper providing high as needed in non-selective preparation for the chemical-mechanical polishing compositions of the inventive method removes speedWith defect performance defect counting��200 of 0.1 ��m (size >) improved.
The method that the present invention is used for being carried out by substrate chemically machinery polished is applicable to carry out chemically machinery polished to containing copper base. The present invention is specially adapted to the semiconductor wafer to having copper-connection for substrate carries out the method for chemically machinery polished and carries out chemically machinery polished.
The substrate using the inventive method to carry out polishing also optionally comprises the additional material being selected from lower group: the TEOS (PETEOS) of phosphosilicate glass (PSG), boron-phosphosilicate glass (BPSG), the silicate glass (USG) not adulterated, spin-coating glass (spin-on-glass, SOG), tetraethyl orthosilicate (TEOS), plasma enhancing, flowable oxide (FOx), high density plasma CVD (HDPCVD) oxide compound and tantalum nitride (TaN). Preferably, it may also be useful to the substrate that the inventive method carries out polishing also comprises the additional material being selected from TaN and TEOS.
Preferably, the water being used as initial component in the chemical-mechanical polishing compositions used in the chemical mechanical polishing method of the present invention is at least one in deionized water and distilled water, to limit subsidiary impurity.
The abrasive material of the chemical-mechanical polishing compositions being suitable for chemical mechanical polishing method of the present invention comprises: such as inorganic oxide, inorganic hydroxide, inorganic hydrogen oxidation oxide (hydroxideoxides), metal boride, metallic carbide, metal nitride, polymer beads and comprise the mixture of above-mentioned at least one. Suitable inorganic oxide comprises: such as silicon-dioxide (SiO2), aluminum oxide (Al2O3), zirconium white (ZrO2), cerium dioxide (CeO2), manganese oxide (MnO2), titanium oxide (TiO2), or comprise the combination of the above-mentioned oxide compound of at least one. If needed, it is possible to use the improved form of these inorganic oxides, the inorganic oxide particles of such as organic polymer coating and the particle of inorganics coating. Suitable metallic carbide, boride and nitride comprise: such as silicon carbide, silicon nitride, carbonitride of silicium (SiCN), norbide, wolfram varbide, zirconium carbide, aluminum boride, tantalum carbide, titanium carbide or the combination of at least one comprised in above-mentioned metallic carbide, metal boride and metal nitride. Preferably, abrasive material used is colloidal silica abrasive. More preferably, the abrasive material used colloidal silica that to be median size be 1-200 nanometer (being more preferably 1-100 nanometer, it is most preferred that be 25-75 nanometer), described median size is measured by well-known light scattering technique.
Better comprising the abrasive material of 0.1-20 weight % for the chemical-mechanical polishing compositions of the chemical mechanical polishing method of the present invention, better comprise the abrasive material of 0.5-15 weight %, the abrasive material preferably including 10-15% is as initial component. Preferably, described abrasive material is colloided silica abrasive material. Most preferably, the mean particle size that the chemical-mechanical polishing compositions of the present invention comprises 10-15 weight % is that the colloidal silica abrasive of 25-75 nanometer is as initial component.
The complexing agent for copper is comprised as initial component for the chemical-mechanical polishing compositions of the chemical mechanical polishing method of the present invention. think that complexing agent can promote that copper is removed from substrate. preferably, it may also be useful to chemical-mechanical polishing compositions comprise better 0.1 to the 1 weight % of 0.01 to 15 weight %(, best 0.1 to 0.5 weight %) complexing agent as initial component. complexing agent comprises: such as acetic acid, citric acid, methyl aceto acetate, oxyacetic acid, lactic acid, oxysuccinic acid, oxalic acid, Whitfield's ointment, Thiocarb, succsinic acid, tartrate, Thiovanic acid, glycine, L-Ala, aspartic acid, quadrol, trimethyl diamine, propanedioic acid, pentanedioic acid, 3-hydroxybutyrate, propionic acid, phthalic acid, m-phthalic acid, 3-hydroxyl Whitfield's ointment, 3.5-dihydroxy salicylic acid, gallic acid, glyconic acid, pyrocatechol, pyrogallol, tannic acid, comprise their salt and mixture. preferably, complexing agent used is selected from: acetic acid, citric acid, methyl aceto acetate, oxyacetic acid, lactic acid, oxysuccinic acid, oxalic acid and their combination. most preferably, complexing agent used is citric acid.
Chemical-mechanical polishing compositions for the chemical mechanical polishing method of the present invention comprises inhibitor as initial component: think that inhibitor can protect the copper at substrate surface to avoid static etching in operation. Preferably, it may also be useful to chemical-mechanical polishing compositions comprise 0.02 to 5 weight %(more preferably 0.05 to 2 weight %, be preferably 0.05 to 1 weight %) inhibitor as initial component. Inhibitor used optionally comprises the mixture of inhibitor. Inhibitor used is preferably azoles (azole) inhibitor. More preferably, inhibitor used is selected from the Azole inhibitors of lower group: benzotriazole (BTA), mercaptobenzothiazole (MBT), tolyl-triazole and imidazoles. Most preferably, described inhibitor is BTA.
Chemical-mechanical polishing compositions for the chemical mechanical polishing method of the present invention comprises P contained compound as initial component: think that P contained compound can promote that copper removes the quickening of speed. preferably, chemical-mechanical polishing compositions used comprises the better 0.05-3 weight % of 0.01-5 weight %(, better 0.05-0.5 weight %, best 0.05-0.2 weight %) P contained compound. the any compound containing phosphorus atom is referred to herein with term " P contained compound " used in appended claims. preferably, P contained compound used is selected from: phosphoric acid class, tetra-sodium class, Tripyrophosphoric acid class, phosphonic acid based, phosphine oxide, phosphine sulfide, positive phosphine (phosphorinane), phosphonic acid based, phosphorous acid class and phosphonous acid class, comprise they acid, salt, nitration mixture salt, ester, partially ester, mixed ester and their mixture, such as phosphoric acid. more preferably, P contained compound used is selected from: zinc phosphate, zinc pyrophosphate, Tripyrophosphoric acid zinc, zinc phosphonate, ammonium phosphate, ammonium pyrophosphate, ammonium polyphosphate, phosphonic acids ammonium, Secondary ammonium phosphate, tetra-sodium hydrogen two ammonium, Tripyrophosphoric acid hydrogen two ammonium, phosphonic acids hydrogen two ammonium, potassiumphosphate, dipotassium hydrogen phosphate, phosphoguanidine, tetra-sodium guanidine, Tripyrophosphoric acid guanidine, phosphonic acids guanidine, tertiary iron phosphate, ferric pyrophosphate, Tripyrophosphoric acid iron, phosphonic acids iron, Cerium monophosphate, cerous pyrophosphate, Tripyrophosphoric acid cerium, phosphonic acids cerium, phosphoric acid quadrol, piperazine phosphate, piperazine pyrophosphate, phosphonic acids piperazine, melamine phosphate, phosphoric acid hydrogen two (trimeric cyanamide), melamine pyrophosphate, melamine polyphosphate, phosphonic acids trimeric cyanamide, phosphoric acid melam, tetra-sodium melam, Tripyrophosphoric acid melam, phosphonic acids melam, phosphoric acid melem, tetra-sodium melem, Tripyrophosphoric acid melem, phosphonic acids melem, phosphoric acid dicyano diamide, Ureaphil, comprises their acid, salt, nitration mixture salt, ester, inclined ester, mixed ester, and their mixture. most preferably, the at least one that P contained compound used is selected from lower group: potassiumphosphate is (such as, Tripotassium phosphate, dipotassium hydrogen phosphate, potassium primary phosphate and their mixture), such as, ammonium phosphate (triammonium phosphate, Secondary ammonium phosphate, primary ammonium phosphate and their mixture) and phosphoric acid. excessive ammonium phosphate can introduce the free ammonium of not desired amount in the solution. excessive free ammonium can attack copper, causes coarse copper surface. the phosphoric acid added and Free alkali metal (such as potassium) reaction in��situ are to form effective especially potassium phosphate salt and dipotassium hydrogen phosphate salt.
Chemical-mechanical polishing compositions for chemical mechanical polishing method of the present invention comprises Polyvinylpyrolidone (PVP) as initial component. Preferably, chemical-mechanical polishing compositions used comprises 0.001 to 3 weight %(and is more preferably 0.05 to 1.5 weight %, it is most preferred that be 0.1 to 1 weight %) Polyvinylpyrolidone (PVP) as initial component.
The weight-average molecular weight of Polyvinylpyrolidone (PVP) used is preferably 1000-1000000. For the object of this specification sheets, weight-average molecular weight represents the molecular weight by gel permeation chromatography measurement. The weight-average molecular weight of described slurries is more preferably 1000-500000, it is most preferred that weight-average molecular weight be 2500-50000. Such as, weight-average molecular weight is that the Polyvinylpyrolidone (PVP) of 12000-20000 has been proved to be effective especially.
Preferably, the chemical-mechanical polishing compositions for chemical mechanical polishing method of the present invention comprises guanidine class thing as initial component, and described guanidine class thing is selected from guanidine, guanidine derivative, guanidine salt and their mixture. More preferably, guanidine class thing used is selected from Guanidinium carbonate and Guanidinium hydrochloride. Most preferably, guanidine class thing used is Guanidinium hydrochloride.
Preferably, chemical-mechanical polishing compositions for chemical mechanical polishing method of the present invention comprises > 0.1-1 weight %(is more preferably 0.25-1 weight %; Most preferably be 0.3-0.5 weight %) Histidine and > 0.1-1 weight %(is more preferably 0.25-1 weight %; Most preferably be 0.3-0.5 weight %) guanidine class thing as initial component, more preferably, wherein, described guanidine class thing is selected from guanidine, guanidine derivative, guanidine salt and their mixture (described guanidine class thing is Guanidinium hydrochloride). More preferably, chemical-mechanical polishing compositions for chemical mechanical polishing method of the present invention comprises > 0.1-1 weight %(is more preferably 0.25-1 weight %; Most preferably be 0.3-0.5 weight %) Histidine and > 0.1-1 weight %(is more preferably 0.25-1 weight %; Most preferably be 0.3-0.5 weight %) guanidine class thing as initial component, more preferably, wherein, described guanidine class thing is selected from guanidine, guanidine derivative, guanidine salt and their mixture (described guanidine class thing is Guanidinium hydrochloride); And be included in chemical-mechanical polishing compositions as the Histidine of initial component and the quality of guanidine class thing have��10%(is more preferably��5%; Most preferably be��1%) difference.
Chemical-mechanical polishing compositions for chemical mechanical polishing method of the present invention comprises oxygenant as initial component. Preferably, chemical-mechanical polishing compositions used comprises 0-25 weight %(and is more preferably 0.1-10 weight %, it is most preferred that be 0.1-5 weight %) oxygenant as initial component. Preferably, oxygenant used is selected from: hydrogen peroxide (H2O2), single persulphate, iodate, cross magnesium phthalate, peracetic acid and other peracid, persulphate, bromate, periodate, nitrate, molysite, cerium salt, Mn (III) salt, Mn (IV) salt and Mn (VI) salt, silver salt, mantoquita, chromic salts, cobalt salt, halogen, hypochlorite and their mixture. Most preferably, oxygenant used is hydrogen peroxide. When chemical-mechanical polishing compositions comprises oxygenant (such as the hydrogen peroxide) of instability time, it is preferable that when in use oxygenant is mixed in described chemical-mechanical polishing compositions.
Chemical-mechanical polishing compositions for chemical mechanical polishing method of the present invention comprises flow agent as initial component. Flow agent used can comprise muriate. Preferred flow agent is ammonium chloride. Preferably, chemical-mechanical polishing compositions of the present invention comprises 0-0.1 weight %(and is more preferably 0.01-0.1 weight %, it is most preferred that be 0.01-0.05 weight %) ammonium chloride as initial component. Think and introduce the appearance that ammonium chloride can improve polishing substrate as the initial component of chemical-mechanical polishing compositions used, and speed can be removed promote that copper remove from substrate by increasing copper.
Chemical-mechanical polishing compositions for chemical mechanical polishing method of the present invention optionally comprises biocide as initial component. Preferably, chemical-mechanical polishing compositions of the present invention comprises 0-0.01 weight %(and is more preferably 0.001-0.01 weight %) biocide as initial component. Preferably, chemical-mechanical polishing compositions used comprises biocide (such as isothiazolinone derivatives) as initial component. Such as, preferred isothiazolinone derivatives comprises: such as, and methyl-4-isothiazoline-3-ketone and CMIT (comprise the Kao Dekesi (Kordex) of 9.5-9.9 weight % methyl-4-isothiazoline-3-ketoneTMMLX, and comprise the Carson (Kathon) of the mixture of methyl-4-isothiazoline-3-ketone and CMITTMICPIII, all can purchased from ROHM AND HAAS company (RohmandHaasCompany)).
For chemical mechanical polishing method of the present invention chemical-mechanical polishing compositions pH value be preferably 8-12(be more preferably 9-11, it is most preferred that be 10-11). It is applicable to regulate the acid of the pH of chemical-mechanical polishing compositions to comprise such as: nitric acid, sulfuric acid and hydrochloric acid. It is applicable to regulate the alkali of the pH of chemical-mechanical polishing compositions to comprise: such as, ammonium hydroxide, potassium hydroxide, tetramethyl ammonium hydroxide and supercarbonate, it is preferable to tetramethyl ammonium hydroxide. Preferably, the potassium hydroxide that the chemical-mechanical polishing compositions of the present invention comprises 0.1-1 weight % is as initial component.
Chemical-mechanical polishing compositions for chemical mechanical polishing method of the present invention also optionally comprises the additional additive being selected from defoamer, dispersion agent, tensio-active agent and buffer reagent.
Preferably, preferably, the method for chemically machinery polished of the present invention comprises: providing substrate, described substrate comprises copper (described substrate is the semiconductor chip comprising copper-connection); Thering is provided a kind of chemical mechanical polishing pulp composition, it comprises following component as initial component: water; 0.1-20 weight %(be preferably 0.5-15 weight %, it is more preferable to be 10-15 weight %) preferably, abrasive material (described abrasive material is mean particle size is the colloidal silica abrasive of 25-75 nanometer); 0.01-15 weight %(be preferably 0.1-1 weight %, it is more preferable to be 0.01-0.5 weight %) preferably, complexing agent (described complexing agent is citric acid); 0.02-5 weight %(be preferably 0.05-2 weight %, it is more preferable to be 0.05-1 weight %) preferably, inhibitor (described inhibitor is benzotriazole); 0.01-5 weight %(be preferably 0.05-3 weight %, it is more preferable to be 0.05-0.5 weight %, it is most preferred that be 0.05-0.2 weight %) preferably, P contained compound (described P contained compound is phosphoric acid); 0.001-3 weight %(is preferably 0.05-1.5 weight %, it is more preferable to be 0.1-1 weight %) Polyvinylpyrolidone (PVP) (preferably, the weight-average molecular weight of described Polyvinylpyrolidone (PVP) is that 2500-50000(is more preferably 12000-20000)); > 0.1-1 weight %(be preferably 0.25-1 weight %, it is more preferable to be 0.25-0.6 weight %) Histidine; > 0.1-1 weight %(preferably 0.25-1 weight %, be more preferably 0.25-0.6 weight %) guanidine class thing, wherein, described guanidine class thing is selected from guanidine, guanidine derivative, guanidine salt and their mixture (preferably, described guanidine class thing is Guanidinium hydrochloride) (preferably, be included in chemical-mechanical polishing compositions as the Histidine of initial component and the quality of Guanidinium hydrochloride have��10%(is more preferably��5%; Most preferably be��1%) difference); 0-25 weight %(be preferably 0.1-10 weight %, it is more preferable to be 0.1-5 weight %) optional oxygenant preferably, (described oxygenant is H2O2); Preferably, the optional flow agent (described flow agent is ammonium chloride) that 0-0.1 weight % (is preferably 0.01-0.1 weight %, it is more preferable to be 0.01-0.05 weight %); 0-0.01 weight %(be preferably 0.001-0.01 weight %) optional biocide; Optional pH adjusting agent (being preferably the pH adjusting agent of 0.1-1 weight %, described pH adjusting agent is potassium hydroxide); The pH value of described chemical mechanical polishing pulp composition is that 9-11(is preferably 10-11); The chemical mechanical polishing pads with glazed surface is provided; Interface between described chemical mechanical polishing pads and substrate or near interface, be assigned on described chemical mechanical polishing pads by described chemical mechanical polishing pulp composition; Dynamically contact is set up with the interface of the down force of 0.69-34.5 kPa between the glazed surface and substrate of chemical mechanical polishing pads; Described substrate is polished; Preferably, and (copper of described chemical-mechanical polishing compositions removes speed (recording under the polishing condition shown in embodiment) to remove part copper from substrate/ minute (be more preferably/ minute), and size after the polishing that produces of described chemical-mechanical polishing compositions > the SP1 defect counting��200(of 0.1 micron (recording under the polishing condition shown in embodiment) is more preferably��100)). Preferably, described substrate also comprises TEOS, TEOS is removed from substrate at least partially, and the copper of described chemical-mechanical polishing compositions is removed selectivity (measuring under the polishing condition shown in embodiment) that speed/TEOS removes speed for 1:1 to 5:1(and is more preferably 1:1 to 3:1). Preferably, described substrate also comprises TaN, TaN is removed from substrate at least partially, and the copper of described chemical-mechanical polishing compositions is removed selectivity (measuring under the polishing condition shown in embodiment) that speed/TaN removes speed for 1:1 to 5:1(and is more preferably 2:1 to 4:1).
Preferably, preferably, the method for chemically machinery polished of the present invention comprises: providing substrate, described substrate comprises copper (described substrate is the semiconductor chip comprising copper-connection); Thering is provided a kind of chemical mechanical polishing pulp composition, it comprises following component as initial component: water; The abrasive material of 10-15 weight %, described abrasive material is mean particle size is the colloidal silica abrasive of 25-75 nanometer; The complexing agent of 0.01-0.5 weight %, described complexing agent is citric acid; The inhibitor of 0.05-1 weight %, described inhibitor is benzotriazole; The P contained compound of 0.05-0.2 weight %, described P contained compound is phosphoric acid; The Polyvinylpyrolidone (PVP) of 0.1-1 weight %, the weight-average molecular weight of described Polyvinylpyrolidone (PVP) is 12000-20000; The Histidine of 0.25-0.6 weight %; The Guanidinium hydrochloride of 0.25-0.6 weight %; The oxygenant of 0.1-5 weight %, described oxygenant is H2O2; The flow agent of 0.01-0.05 weight %, described flow agent is ammonium chloride; The biocide of 0.001-0.01 weight %; With the pH adjusting agent of 0.1-1 weight %, described pH adjusting agent is potassium hydroxide; It is included in chemical-mechanical polishing compositions as the Histidine of initial component and the quality of Guanidinium hydrochloride and has��the difference of 10%; The chemical mechanical polishing pads with glazed surface is provided; Interface between described chemical mechanical polishing pads and substrate or near interface, be assigned on described chemical mechanical polishing pads by described chemical mechanical polishing pulp composition; And set up dynamically contact with the interface of the down force of 0.69-34.5 kPa between the glazed surface and substrate of chemical mechanical polishing pads; Described substrate is polished; And from substrate remove a part copper. Preferably, on the polishing machine of 200 millimeters under following operational condition, the copper of described chemical-mechanical polishing compositions removes speed/ minute (be more preferably/ minute), and size after polishing > the SP1 defect counting��200(of 0.1 micron is more preferably��100): platen rotating speed 93 revs/min, carrier velocity 87 revs/min, flow 300 ml/min of chemical-mechanical polishing compositions, apply the nominal down force of 11.7 kPas, described polishing machine uses chemical mechanical polishing pads, and it comprises the non-woven subpad of the polyurethane polishing layer containing the hollow core particulate of polymkeric substance and polyurethane impregnated.
Some embodiments of the present invention will be described now in the examples below in detail.
Embodiment
Chemical-mechanical polishing compositions
The chemical-mechanical polishing compositions (CMPC's) of all tests comprises following component as initial component: the weight-average molecular weight of the ammonium chloride of 0.04 weight %, the benzotriazole of 0.06 weight %, 0.4 weight % be 15000 Polyvinylpyrolidone (PVP), the citric acid of 0.3 weight %, the phosphoric acid of 0.1 weight %, the biocide (Kao Dekesi (Kordex) of 0.005 weight %TMMLX, purchased from ROHM AND HAAS company, comprises 9.5-9.9 weight % methyl-4-isothiazoline-3-ketone), the potassium hydroxide of 0.4 weight %, 14 weight % abrasive material (II1501-50 colloidal silica, mean particle size is 50 nanometers, and AZ electronic material company (AZElectronicMaterials) produces, purchased from ROHM AND HAAS electronic material CMP company limited) and the hydrogen peroxide of 0.4 weight %. The additional initial component (if any) that described CMPCs comprises is as shown in table 1. Chemical-mechanical polishing compositions A-C is comparative formulations, within the scope of claimed the present invention.
Table 1
Polishing is tested
Copper coating wafer, TaN coating wafer and TEOS coating wafer are carried out polishing experiments by the chemical-mechanical polishing compositions described in use table 1. What use Applied Materials Inc (AppliedMaterials, Inc.) is equipped with ISRM detector system200mm polishing machine, it may also be useful to VisionPadTM3100(has 1010 depressions (groves) and SP2310 subpad) polyurethane polishing pad (purchased from ROHM AND HAAS electronic material CMP company limited) carries out polishing experiments under the following conditions: downward pressure is 1.7psi(11.7 kPa), the flow of chemical-mechanical polishing compositions is 300 ml/min, platen rotating speed is 93 revs/min, carrier velocity be 87 revs/min and apart from polishing pad center 4.4 " slurries dropping point. UseAD3BG150840 diamond pad conditioner device (can company (KinikCompany) purchased from Ke Ni) conditioning polishing pad. Copper shown in table 2 is removed speed and is used Jordan paddy (JordanValley) JVX-5200T to measure measuring apparatus. The removal speed of TEOS and TaN shown in table 2 records with the use of the film thickness before and after KLA-TencorFX200 tolerance measuring apparatus polishing. Use the SP1 purchased from KLA Tyke company (KLA-Tencor) to measure equipment and the copper defect of size >=0.1 micron is carried out defect counting analysis.
Table 2
The defect sum of size >=0.1 micron on the copper coating wafer of polishing.
Claims (9)
1. the method being used for being carried out by substrate chemically machinery polished, the method comprises:
Thering is provided substrate, described substrate comprises copper;
Thering is provided a kind of chemical mechanical polishing pulp composition, it comprises following material as initial component:
Water;
The median size of 10-15 weight % is the colloidal silica abrasive of 25-75nm;
The complexing agent of 0.1-0.5 weight %, wherein said complexing agent is citric acid;
The inhibitor of 0.02-5 weight %;
The P contained compound of 0.01-5 weight %;
The Polyvinylpyrolidone (PVP) of 0.001-3 weight %;
The Histidine of 0.25-0.6 weight %;
The guanidine class thing of 0.25-0.6 weight %, described guanidine class thing is selected from guanidine, guanidine derivative, guanidine salt and their mixture;
The optional oxygenant of 0-25 weight %;
The optional flow agent of 0-0.1 weight %;
The optional biocide of 0-0.01 weight %; With
Optional pH adjusting agent;
The pH value of described chemical mechanical polishing pulp composition is 9-11;
The chemical mechanical polishing pads with glazed surface is provided;
Interface between described chemical mechanical polishing pads and substrate or near interface, be assigned on described chemical mechanical polishing pads by described chemical mechanical polishing pulp composition; And
Dynamically contact is set up with the interface of the down force of 0.69-34.5kPa between the glazed surface and substrate of chemical mechanical polishing pads;
Described substrate is polished, and the copper removal speed of described chemical-mechanical polishing compositions >=, and size after the polishing of described chemical-mechanical polishing compositions > SP1 defect counting��200 of 0.1 micron; And from substrate remove a part copper.
2. the method for claim 1, it is characterised in that, described substrate comprises tetraethyl orthosilicate further, and tetraethyl orthosilicate is removed from described substrate at least partially; It is 1:1-5:1 that the copper of described chemical-mechanical polishing compositions removes the selectivity of speed/tetraethyl orthosilicate removal speed.
3. the method for claim 1, it is characterised in that, described substrate comprises TaN further, and TaN is removed from described substrate at least partially; It is 1:1-5:1 that the copper of described chemical-mechanical polishing compositions removes the selectivity of speed/TaN removal speed.
4. the method for claim 1, it is characterised in that, described chemical-mechanical polishing compositions comprises following material as initial component:
Water;
The abrasive material of 10-15 weight %, described abrasive material is mean particle size is the colloidal silica abrasive of 25-75 nanometer;
The complexing agent of 0.1-0.5 weight %, described complexing agent is citric acid;
The inhibitor of 0.05-2 weight %, described inhibitor is benzotriazole;
The P contained compound of 0.05-3 weight %, described P contained compound is phosphoric acid;
The Polyvinylpyrolidone (PVP) of 0.05-1.5 weight %, the weight-average molecular weight of described Polyvinylpyrolidone (PVP) is 2500-50000;
The Histidine of 0.25-0.6 weight %;
The guanidine class thing of 0.25-0.6 weight %, described guanidine class thing is selected from guanidine, guanidine derivative, guanidine salt and their mixture;
The oxygenant of 0.1-10 weight %, described oxygenant is H2O2;
The flow agent of 0.01-0.1 weight %, described flow agent is ammonium chloride;
The biocide of 0.001-0.01 weight %; With
The pH adjusting agent of 0.1-1 weight %, described pH adjusting agent is potassium hydroxide.
5. method as claimed in claim 4, it is characterised in that, on the polishing machine of 200 millimeters under following operational condition, the copper removal speed of described chemical-mechanical polishing compositions >=And size after polishing > SP1 defect counting��200 of 0.1 micron: platen rotating speed 93 revs/min, carrier velocity 87 revs/min, flow 300 ml/min of chemical-mechanical polishing compositions, apply the nominal down force of 11.7 kPas, described polishing machine uses chemical mechanical polishing pads, and it comprises the non-woven subpad of the polyurethane polishing layer containing the hollow core particulate of polymkeric substance and polyurethane impregnated.
6. method as claimed in claim 5, it is characterised in that, described substrate comprises tetraethyl orthosilicate further, and tetraethyl orthosilicate is removed from described substrate at least partially; And, on the polishing machine of 200 millimeters under following operational condition, it is 1:1 to 5:1 that the copper of described chemical-mechanical polishing compositions removes the selectivity of speed/tetraethyl orthosilicate removal speed: platen rotating speed 93 revs/min, carrier velocity 87 revs/min, flow 300 ml/min of chemical-mechanical polishing compositions, apply the nominal down force of 11.7 kPas, described polishing machine uses chemical mechanical polishing pads, and it comprises the non-woven subpad of the polyurethane polishing layer containing the hollow core particulate of polymkeric substance and polyurethane impregnated.
7. method as claimed in claim 5, it is characterised in that, described substrate comprises TaN further, and TaN is removed from described substrate at least partially; And, on the polishing machine of 200 millimeters under following operational condition, it is 1:1 to 5:1 that the copper of described chemical-mechanical polishing compositions removes the selectivity of speed/TaN removal speed: platen rotating speed 93 revs/min, carrier velocity 87 revs/min, flow 300 ml/min of chemical-mechanical polishing compositions, apply the nominal down force of 11.7 kPas, described polishing machine uses chemical mechanical polishing pads, and it comprises the non-woven subpad of the polyurethane polishing layer containing the hollow core particulate of polymkeric substance and polyurethane impregnated.
8. the method for claim 1, it is characterised in that, described chemical-mechanical polishing compositions comprises following material as initial component:
Water;
The abrasive material of 10-15 weight %, described abrasive material is mean particle size is the colloidal silica abrasive of 25-75 nanometer;
The complexing agent of 0.1-0.5 weight %, described complexing agent is citric acid;
The inhibitor of 0.05-1 weight %, described inhibitor is benzotriazole;
The P contained compound of 0.05-0.2 weight %, described P contained compound is phosphoric acid;
The Polyvinylpyrolidone (PVP) of 0.1-1 weight %, the weight-average molecular weight of described Polyvinylpyrolidone (PVP) is 12000-20000;
The Histidine of 0.25-0.6 weight %;
The guanidine class thing of 0.25-0.6 weight %, described guanidine class thing is Guanidinium hydrochloride;
The oxygenant of 0.1-5 weight %, described oxygenant is H2O2;
The flow agent of 0.01-0.05 weight %, wherein, described flow agent is ammonium chloride;
The biocide of 0.001-0.01 weight %; With
The pH adjusting agent of 0.1-1 weight %, wherein, described pH adjusting agent is potassium hydroxide;
It is included in chemical-mechanical polishing compositions as the Histidine of initial component and the quality of Guanidinium hydrochloride and has��the difference of 10%.
9. method as claimed in claim 8, it is characterised in that, on the polishing machine of 200 millimeters under following operational condition, the copper removal speed of described chemical-mechanical polishing compositions >=And size after polishing > SP1 defect counting��200 of 0.1 micron: platen rotating speed 93 revs/min, carrier velocity 87 revs/min, flow 300 ml/min of chemical-mechanical polishing compositions, apply the nominal down force of 11.7 kPas, described polishing machine uses chemical mechanical polishing pads, and it comprises the non-woven subpad of the polyurethane polishing layer containing the hollow core particulate of polymkeric substance and polyurethane impregnated.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US13/209,864 | 2011-08-15 | ||
| US13/209,864 US20130045599A1 (en) | 2011-08-15 | 2011-08-15 | Method for chemical mechanical polishing copper |
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| CN102950537A CN102950537A (en) | 2013-03-06 |
| CN102950537B true CN102950537B (en) | 2016-06-01 |
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| US (1) | US20130045599A1 (en) |
| JP (1) | JP6041095B2 (en) |
| KR (1) | KR101945221B1 (en) |
| CN (1) | CN102950537B (en) |
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| JP6035346B2 (en) * | 2011-12-21 | 2016-11-30 | ビーエーエスエフ ソシエタス・ヨーロピアＢａｓｆ Ｓｅ | Method for manufacturing semiconductor device and method for using CMP composition |
| US9299585B2 (en) * | 2014-07-28 | 2016-03-29 | Rohm And Haas Electronic Materials Cmp Holdings, Inc. | Method for chemical mechanical polishing substrates containing ruthenium and copper |
| CN106916536B (en) * | 2015-12-25 | 2021-04-20 | 安集微电子（上海）有限公司 | Alkaline chemical mechanical polishing solution |
| CN107145614B (en) * | 2016-03-01 | 2020-06-30 | 中国科学院微电子研究所 | CMP process simulation method and system |
| US10377921B2 (en) * | 2017-09-21 | 2019-08-13 | Rohm and Haas Electronics Materials CMP Holdings, Inc. | Chemical mechanical polishing method for cobalt |
| US20200095502A1 (en) * | 2018-09-26 | 2020-03-26 | Versum Materials Us, Llc | High Oxide VS Nitride Selectivity, Low And Uniform Oxide Trench Dishing In Shallow Trench Isolation(STI) Chemical Mechanical Planarization Polishing(CMP) |
| WO2020091242A1 (en) * | 2018-10-31 | 2020-05-07 | 영창케미칼 주식회사 | Slurry composition for polishing copper barrier layer |
| CN114341287B (en) * | 2019-09-04 | 2024-03-15 | Cmc材料有限责任公司 | Composition and method for polysilicon chemical mechanical polishing |
| JP7409899B2 (en) * | 2020-02-18 | 2024-01-09 | 株式会社フジミインコーポレーテッド | Polishing composition, polishing method, and semiconductor substrate manufacturing method |
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| US20100159807A1 (en) * | 2008-12-22 | 2010-06-24 | Jinru Bian | Polymeric barrier removal polishing slurry |
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- 2011-08-15 US US13/209,864 patent/US20130045599A1/en not_active Abandoned
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- 2012-08-03 JP JP2012173340A patent/JP6041095B2/en active Active
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- 2012-08-09 DE DE102012015824A patent/DE102012015824A1/en not_active Withdrawn
- 2012-08-14 CN CN201210289359.6A patent/CN102950537B/en active Active
- 2012-08-14 KR KR1020120089008A patent/KR101945221B1/en active IP Right Grant
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| CN1900206A (en) * | 2005-07-21 | 2007-01-24 | 安集微电子（上海）有限公司 | Chemical and mechanical polishing liquid and its use |
| CN1927975A (en) * | 2005-09-08 | 2007-03-14 | 罗门哈斯电子材料Cmp控股股份有限公司 | Polishing slurry capable of removing polymer barrier layer |
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Also Published As
| Publication number | Publication date |
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| TWI594310B (en) | 2017-08-01 |
| DE102012015824A1 (en) | 2013-02-21 |
| JP2013042132A (en) | 2013-02-28 |
| US20130045599A1 (en) | 2013-02-21 |
| CN102950537A (en) | 2013-03-06 |
| JP6041095B2 (en) | 2016-12-07 |
| KR20130020585A (en) | 2013-02-27 |
| FR2979071A1 (en) | 2013-02-22 |
| TW201320173A (en) | 2013-05-16 |
| KR101945221B1 (en) | 2019-02-07 |
| FR2979071B1 (en) | 2016-08-26 |
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